Refining of therapeutic oils



Patented Apr. 12, 1933 UNITED STATES DEFINING F THERAPEUTIC oms William S. Jones, Brooklyn, N. Y., assignor to E. R. Squibb & Sons, New York, N. Y., a corporation of New York No Drawing. Application June 30, 1934, Serial No. 733,331

3 Claims.

This invention relates to, and has for its object the provision of an efiicient method for, the refining of oils-particularly the liver and body oils of halibut, cod, salmon, tuna, black cod,

5 ling, swordfish, and other fish-that are intended for therapeutic use and must therefore be highly purified, in order to be acceptable for internal administration, but are so costly as to make any considerable processing losses prohibi-' tive.

In the practice of this invention, the oil to be refined (which may have been extracted, for instance, from raw or cooked liver) is present dissolved in a solvent-say ethylene dichloride, tri- 16 chlorethylene, or dichlorethylether-that does not dissolve soap, less than five percent its volume of alcohol is added to the solution, and sufficient caustic alkali is added to insure complete saponification of the free fatty acids. Removal of the separated soap and the solvent, leaves the oil, substantially purified of free fatty'acids, acrid substances, and foreign coloring matter. Preferably,, after removal of the soap, the solution is treated with carbon to perfect the purification.

Refining of the oil is thoroughly accomplished by this process, without appreciable loss and without injury to any labile ingredients, such as vitamin A. f

For example, to-400 cc. of a dark solution of 30 halibut-liver oil made by extracting halibut livers with ethylene dichloride, each 100 cc. of solution containing 10 to 20 g. of the oil and 2 g. of free fatty acids, 4 cc. of 95% alcohol is added, the mixture is agitated, 16.0 cc. (an approximately 35 100% excess) of 18 B. sodium hydroxide solution is added, and the mixture is agitated for about ten minutes (during which the solution and the separating soap progressively acquire lighter and darker colors, respectively) and al- 40 lowed to stand for. an hour, the soap having then formed into a floating semi-solid layer. The ethylene dichloride solution is drawn oi! into a cylinder, agitated with an adsorbing earth such as Hyflocel, filtered through paper, and evaporated, yielding a light-amber oil free from soap and from unpleasant taste and odor and having a free-fattyacid content of 0.07%. Agitation of 5 the solution with 2.0 g, of carbon and paper-filtration, just before evaporation, results in further removal of color, giving a light-yellow oil.

It is to be understood that the foregoing example is merely illustrative and by no means lim- 10 itative of the invention, which may be variously otherwise embodied-as with respect to particular oils, solvents, caustic alkalis, adsorbents, and procedures-:within the scope of the appended claims.

I claim:

1. In the process of refining oils, the steps of adding to a solution thereof, in a solvent that does not dissolve soap, some alcohol, the volume of the alcohol added being lws than 5% of the 20 volume of the solution, and adding sufiicient caustic alkali to saponify the free fatty acids, the separating soap removing acrid substances and foreign coloring matter from the oil.

2. In the process of refining halibut-liver oil, the steps of adding to a solution thereof, in asolvent that does not dissolve soap, some alcohol, the volume of the alcohol added being less than 5% of the volume of thesolution, andadding sufficient caustic alkali to saponify the free fatty 3o acids, the separating soap removing acrid substances and foreign coloring matter from the oil.

3. In the process of refining halibut-liver oil, the steps of adding to an ethylene dichloride solution thereof some alcohol, the volume of the alcohol 5 added being less than 5% of the volume of the solution, andadding sufiicient caustic alkali to, saponify the free fatty acids, the separating soap removing acrid substances. and foreign coloring matter from the oil. 40 WILLIAM S. JONES. 

